CN109225152B - Ultrafast high-adsorption-performance cellulose elastic carbon aerogel and preparation method and application thereof - Google Patents
Ultrafast high-adsorption-performance cellulose elastic carbon aerogel and preparation method and application thereof Download PDFInfo
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 41
- 239000001913 cellulose Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000001179 sorption measurement Methods 0.000 claims abstract description 58
- 239000004964 aerogel Substances 0.000 claims abstract description 40
- 229920002749 Bacterial cellulose Polymers 0.000 claims abstract description 39
- 239000005016 bacterial cellulose Substances 0.000 claims abstract description 39
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 24
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 24
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 24
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 24
- 238000001723 curing Methods 0.000 claims abstract description 18
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 238000007710 freezing Methods 0.000 claims abstract description 16
- 230000008014 freezing Effects 0.000 claims abstract description 16
- 238000001291 vacuum drying Methods 0.000 claims abstract description 15
- PTHCMJGKKRQCBF-UHFFFAOYSA-N Cellulose, microcrystalline Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC)C(CO)O1 PTHCMJGKKRQCBF-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
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- 238000000034 method Methods 0.000 claims description 12
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- 239000002609 medium Substances 0.000 claims description 8
- 239000001888 Peptone Substances 0.000 claims description 6
- 108010080698 Peptones Proteins 0.000 claims description 6
- 229940041514 candida albicans extract Drugs 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 6
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 6
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- 238000001354 calcination Methods 0.000 claims description 2
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4868—Cells, spores, bacteria
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Abstract
The invention discloses ultrafast high-adsorption-performance cellulose elastic carbon aerogel and a preparation method and application thereof, and belongs to the field of production of aerogel functional materials. The preparation method comprises the steps of bacterial cellulose synthesis, bacterial cellulose gel film freezing and curing, vacuum drying, PDMS dipping treatment, high-temperature calcination and the like. The bacterial fiber is hydrogel with high water content, is pure and long, can obviously improve the porosity and the flexibility of the aerogel, and the PDMS can endow the aerogel with good elasticity and mechanical toughness. Carbonization in inert nitrogen is favorable to doping of silicon and can increase the specific surface area of aerogel, improves the hydrophobicity on aerogel surface, and then improves adsorption rate and adsorption effect, and the cellulose base carbon aerogel that finally obtains has three-dimensional space network structure and good elasticity recovery, can still bounce back after compressing 85%, can accomplish in 30s the absorption of 90# petrol, and the adsorption capacity can reach 140 ~ 160 times of self quality.
Description
Technical Field
The invention belongs to the field of aerogel functional material production, and particularly relates to ultrafast high-adsorption-performance cellulose elastic carbon aerogel and a preparation method and application thereof.
Background
Aerogels, also known as xerogels, are intact frameworks that remain after removal of the solvent from the gel. The aerogel has the characteristics of low density, large specific surface area, porous structure, high porosity and the like, and can be widely used in the fields of aerospace military industry, filter materials, oil leakage adsorption, high-efficiency catalysis, energy storage and the like. Typically, the density is less than 10mg/cm3The aerogel of (a) may be referred to as an ultra-light aerogel. In recent years, some novel aerogels such as graphene carbon aerogel and the like have been discovered, and have the characteristics of high strength, low density, excellent conductivity and the like, but the achievement of a large amount of ultra-light elastic aerogel is still a challenge.
At present, the adsorption method is considered to be the most effective treatment method for treating water pollution caused by crude oil leakage or organic solvent due to the characteristics of simple operation, small pollution, low energy consumption and the like. However, the traditional adsorbent materials have the bottleneck problems of low adsorption efficiency, long adsorption time, poor cycle performance and the like. Therefore, development of an ideal adsorbent having excellent adsorption selectivity, high adsorption speed, high adsorption amount, low cost and recyclability is urgently required. In recent years, some graphene-based aerogel materials have attracted much attention in the fields of oil leakage adsorption and the like due to their inherent characteristics such as hydrophobicity and high specific surface area. However, the existing preparation process of graphene-based carbon aerogel mostly uses higher reaction temperature and pressure, or uses non-green chemical reagents, and the high energy consumption and the use of a large amount of reagents are against the vision of people on green environmental protection and cost. It would therefore be desirable to produce high performance carbon aerogels on a renewable resource basis in a more efficient, sustainable process on a large scale to facilitate their practical application.
Based on the current situations that harmful substances are involved in the preparation process of some carbon aerogels at present, the equipment is complex, the process is complicated, and the performance is not high, a sustainable method is needed to be found for mass production of the ultra-fast high-adsorption-performance carbon aerogels, so that the ultra-fast high-adsorption-performance carbon aerogels have high adsorption speed and high elasticity, the high added value is given, and the requirement of crude oil adsorption is met.
Disclosure of Invention
In order to overcome the defects and shortcomings of the existing carbon aerogel production technology, the invention mainly aims to provide a preparation method of cellulose elastic carbon aerogel with ultra-fast high adsorption performance.
According to the invention, the massive biological cellulose membrane is subjected to liquid nitrogen freezing treatment to keep the massive biological cellulose membrane in a three-dimensional structure; and then carrying out freeze drying treatment, soaking the aerogel in PDMS prepolymer, then curing in an oven, and finally carrying out high-temperature calcination treatment by using argon gas to obtain the ultrafast high-adsorption cellulose elastic carbon aerogel.
The invention also aims to provide the ultrafast high-adsorption cellulose elastic carbon aerogel obtained by the preparation method.
The invention further aims to provide application of the ultrafast high-adsorption cellulose elastic carbon aerogel.
The purpose of the invention is realized by the following technical scheme:
a preparation method of ultrafast high-adsorption cellulose elastic carbon aerogel comprises the following steps:
(1) and (3) synthesis of bacterial cellulose: inoculating acetobacter xylinum to a fermentation culture medium containing coconuts, and fermenting and biologically synthesizing a bacterial cellulose gel liquid membrane under the conditions of 35-38 ℃ and 40-50% relative humidity RH;
(2) freezing and vacuum drying treatment: freezing and solidifying the bacterial cellulose aerogel film obtained in the step (1) by using liquid nitrogen, and then carrying out vacuum drying treatment on the block-shaped module to obtain the bacterial cellulose aerogel;
(3) and (3) PDMS dipping treatment: soaking the bacterial cellulose aerogel obtained in the step (2) in PDMS prepolymer, enabling bubbles in the mixed solution to float to the surface and break by means of vacuumizing, and then putting the mixed solution into an oven;
(4) high-temperature calcination: and (4) performing high-temperature calcination treatment on the material obtained in the step (3), and then cooling to obtain the ultrafast high-adsorption cellulose elastic carbon aerogel.
The content of the coconut in the fermentation medium containing the coconut in the step (1) is 20 g/L, wherein the solid content of the coconut is 50-60%.
The fermentation medium comprises peptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1.0 g/L, and Na2HPO4：3.0g/L，MgSO4：0.4g/L。
The thickness of the bacterial cellulose gel liquid film in the step (1) is 10-20 mm.
The temperature of the liquid nitrogen freezing and curing treatment in the step (2) is-195 ℃, and the curing time is 10-20 min; the vacuum drying temperature is-45 ℃, the drying time is 60-72 hours, and the vacuum degree is 5-20 Pa.
The PDMS prepolymer in step (3) refers to a mixture of a silicone rubber prepolymer (Sylgard 184) and a curing agent (dow corning, USA) in a ratio of 10: 1, and mixing. And vacuumizing for 30-60 min. Thermally curing for 1-4 h in an oven at 60-80 ℃.
The high-temperature calcination treatment in the step (4) is carried out under the protection of nitrogen, the calcination temperature is 500-800 ℃, the temperature is increased to 300-400 ℃ at 2.0-3.0 ℃/min, the temperature is maintained for 60-90 min, the temperature is increased to a target temperature at 4-4.5 ℃/min, the temperature is maintained for 90-120 min, and then the temperature is reduced to the room temperature.
The ultrafast high-adsorption cellulose elastic carbon aerogel is prepared by the preparation method.
The properties of the ultrafast high-adsorption cellulose elastic carbon aerogel are as follows: density: 5-8 mg/cm3(ii) a Compressibility: 78-85%; porosity: 86-92%; specific surface area SBET＝636～682m2(ii)/g; adsorption time for gasoline (90 #): 10-30 s; the adsorption capacity can reach 140-160 times of the self mass.
The ultrafast high-adsorption cellulose elastic carbon aerogel is applied to gasoline adsorption.
The ultrafast high-adsorption-performance cellulose elastic carbon aerogel disclosed by the invention is a strategy of reasonably compounding bacterial cellulose and elastomer polymer PDMS and complementing advantages. The bacterial cellulose is nano-cellulose, has the performance advantages of high purity, high water content, large length-diameter ratio, high Young modulus and the like, and is a typical hydrogel; PDMS is a transparent elastomer with stable structure, and has the characteristics of no toxicity, hydrophobicity, non-flammability and the like. PDMS can be used as a skeleton of elastomer support carbon, so that the PDMS can keep a three-dimensional space structure in the high-temperature calcination process; on the other hand, PDMS is used as a high molecular organic silicon compound, a part of silicon is doped into the amorphous carbon skeleton of the bacterial cellulose in the high-temperature calcination process, and the doping of the silicon can enhance the mechanical toughness of the bacterial cellulose aerogel. The carbonization process can increase the specific surface area and surface hydrophobicity of the aerogel, thereby further increasing the adsorption rate and adsorption amount. The two substances are compounded to prepare the ultrafast high-adsorption cellulose elastic carbon aerogel.
Compared with the prior art, the invention has the following advantages and effects:
the preparation method of the ultrafast high-adsorption cellulose elastic carbon aerogel is simple, and the raw materials are cheap and easy to obtain. The carbon aerogel is obtained by reasonably compounding bacterial cellulose and elastomer PDMS, the advantages of all components are fully utilized, the bacterial fiber is hydrogel with high water content, the fiber is pure and long, the porosity and flexibility of the aerogel can be obviously improved, and the PDMS can endow the aerogel with good elasticity and mechanical toughness. The specific surface area of the aerogel can be increased by carbonizing the aerogel in inert nitrogen, the hydrophobicity of the surface of the aerogel is improved, the adsorption speed and the adsorption effect are further improved, the finally obtained cellulose-based carbon aerogel has a three-dimensional space network structure and good elastic recovery, the cellulose-based carbon aerogel can still rebound after being compressed by 85%, the adsorption on gasoline (90#) can be completed within 30s, and the adsorption capacity can reach 140-160 times of the mass of the aerogel.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
In the invention: the detection of various parameters is carried out according to a national standard detection method and an industrial standard, and specifically comprises the following steps: the porosity (GB/T3366-.
The Acetobacter xylinum used in the examples was Acetobacter xylinum (ATCC 23767).
Example 1
The preparation method of the ultrafast high-adsorption cellulose elastic carbon aerogel provided by the embodiment comprises the following specific preparation steps:
(1) preparation of bacterial cellulose by adding 20 g/L of coconut fruit into fermentation medium (peptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1.0 g/L, Na2HPO4：3.0g/L，MgSO40.4 g/L), inoculating acetobacter xylinum, fermenting and biologically synthesizing a bacterial cellulose gel film with the thickness of 10mm under the conditions that the temperature is 35 ℃ and the relative humidity is 40 percent RH;
(2) freezing and vacuum drying treatment: freezing and curing the bacterial cellulose aerogel film obtained in the step (1) by using liquid nitrogen at the temperature of-195 ℃ for 10min, and then carrying out vacuum drying on the block module for 60h at the temperature of-45 ℃ and the vacuum degree of 5Pa to obtain the bacterial cellulose aerogel;
(3) and (3) PDMS dipping treatment: immersing the bacterial cellulose aerogel obtained in the step (2) in a PDMS prepolymer, wherein the prepolymer is prepared by mixing a silicon rubber prepolymer (Sylgard 184) and a curing agent (Dow Corning, USA) in a ratio of 10: 1, and mixing. Vacuum is applied for 30min to make the bubbles in the mixture float to the surface and break. Then placing the mixture in an oven to be thermally cured for 1h at 60 ℃;
(4) high-temperature calcination: and (4) carrying out high-temperature calcination treatment on the material obtained in the step (3) under the protection of nitrogen. Heating to 300 ℃ at the speed of 2.0 ℃/min, preserving heat for 60min, then heating to 500 ℃ at the speed of 4.0 ℃/min, preserving heat for 90min, and then cooling to room temperature to prepare the ultrafast high-adsorption cellulose elastic carbon aerogel.
The performance detection data of the ultrafast high-adsorption cellulose elastic carbon aerogel of the embodiment are as follows: density: 8mg/cm3(ii) a Compressibility: 78 percent; porosity: 86 percent; specific surface area SBET＝651m2(ii)/g; adsorption time for gasoline (90 #): 30 s; the adsorption capacity can reach 140 times of the self mass.
Example 2
The preparation method of the ultrafast high-adsorption cellulose elastic carbon aerogel provided by the embodiment comprises the following specific preparation steps:
(1) preparation of bacterial cellulose by adding 20 g/L of coconut fruit into fermentation medium (peptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1.0 g/L, Na2HPO4：3.0g/L，MgSO40.4 g/L), inoculating acetobacter xylinum, and fermenting and biologically synthesizing a bacterial cellulose gel liquid film with the thickness of 15mm under the conditions that the temperature is 36 ℃ and the relative humidity is 45 percent RH;
(2) freezing and vacuum drying treatment: freezing and curing the bacterial cellulose aerogel film obtained in the step (1) by using liquid nitrogen at the temperature of minus 195 ℃ for 10min, and then carrying out vacuum drying on the block module for 66h at the temperature of minus 45 ℃ and the vacuum degree of 10Pa to obtain the bacterial cellulose aerogel;
(3) and (3) PDMS dipping treatment: immersing the bacterial cellulose aerogel obtained in the step (2) in a PDMS prepolymer, wherein the prepolymer is prepared by mixing a silicon rubber prepolymer (Sylgard 184) and a curing agent (Dow Corning, USA) in a ratio of 10: 1, and mixing. Vacuum is applied for another 40min to make the bubbles in the mixture float to the surface and break. Then placing the mixture in an oven to be thermally cured for 2 hours at 70 ℃;
(4) high-temperature calcination: and (4) carrying out high-temperature calcination treatment on the material obtained in the step (3) under the protection of nitrogen. Heating to 350 ℃ at the speed of 3.0 ℃/min, preserving heat for 70min, then heating to 600 ℃ at the speed of 4.0 ℃/min, preserving heat for 100min, and then cooling to room temperature to prepare the ultrafast high-adsorption cellulose elastic carbon aerogel.
The performance detection data of the ultrafast high-adsorption cellulose elastic carbon aerogel of the embodiment are as follows: density: 7mg/cm3(ii) a Compressibility: 81 percent; porosity: 88 percent; specific surface area SBET＝636m2(ii)/g; adsorption time for gasoline (90 #): 22 s; the adsorption capacity can reach 148 times of the self mass.
Example 3
The preparation method of the ultrafast high-adsorption cellulose elastic carbon aerogel provided by the embodiment comprises the following specific preparation steps:
(1) preparation of bacterial cellulose by adding 20 g/L of coconut fruit into fermentation medium (peptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1.0 g/L, Na2HPO4：3.0g/L，MgSO40.4 g/L), inoculating acetobacter xylinum, fermenting and biologically synthesizing a bacterial cellulose gel film with the thickness of 20mm under the conditions of the temperature of 37 ℃ and the relative humidity of 48 percent RH;
(2) freezing and vacuum drying treatment: freezing and curing the bacterial cellulose aerogel film obtained in the step (1) by using liquid nitrogen at the temperature of-195 ℃ for 20min, and then carrying out vacuum drying on the block module for 70h at the temperature of-45 ℃ and the vacuum degree of 15Pa to obtain the bacterial cellulose aerogel;
(3) and (3) PDMS dipping treatment: immersing the bacterial cellulose aerogel obtained in the step (2) in a PDMS prepolymer, wherein the prepolymer is prepared by mixing a silicon rubber prepolymer (Sylgard 184) and a curing agent (Dow Corning, USA) in a ratio of 10: 1, and mixing. Vacuum is applied for 50min to make the bubbles in the mixture float to the surface and break. Then putting the mixture into an oven to be thermally cured for 3 hours at 70 ℃;
(4) high-temperature calcination: and (4) carrying out high-temperature calcination treatment on the material obtained in the step (3) under the protection of nitrogen. Heating to 400 ℃ at the speed of 2.5 ℃/min, preserving heat for 80min, heating to 700 ℃ at the speed of 4.5 ℃/min, preserving heat for 110min, and cooling to room temperature to prepare the ultrafast high-adsorption cellulose elastic carbon aerogel.
Ultrafast high-adsorbability fiber of this embodimentPerformance test data of vitamin elastic carbon aerogel: density: 6mg/cm3(ii) a Compressibility: 83 percent; porosity: 90 percent; specific surface area SBET＝667m2(ii)/g; adsorption time for gasoline (90 #): 15 s; the adsorption capacity can reach 153 times of the self mass.
Example 4
The preparation method of the ultrafast high-adsorption cellulose elastic carbon aerogel provided by the embodiment comprises the following specific preparation steps:
(1) preparation of bacterial cellulose by adding 20 g/L of coconut fruit into fermentation medium (peptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1.0 g/L, Na2HPO4：3.0g/L，MgSO40.4 g/L), inoculating acetobacter xylinum, fermenting and biologically synthesizing bacterial cellulose gel membranes with the thickness of 10mm under the conditions of the temperature of 38 ℃ and the relative humidity of 50% RH;
(2) freezing and vacuum drying treatment: freezing and curing the bacterial cellulose aerogel film obtained in the step (1) by using liquid nitrogen at the temperature of minus 195 ℃ for 20min, and then carrying out vacuum drying on the block module for 72h at the temperature of minus 45 ℃ and the vacuum degree of 20Pa to obtain the bacterial cellulose aerogel;
(3) and (3) PDMS dipping treatment: immersing the bacterial cellulose aerogel obtained in the step (2) in a PDMS prepolymer, wherein the prepolymer is prepared by mixing a silicon rubber prepolymer (Sylgard 184) and a curing agent (Dow Corning, USA) in a ratio of 10: 1, and mixing. Vacuum is applied for 60min to make the bubbles in the mixture float to the surface and break. Then putting the mixture into an oven to be thermally cured for 4 hours at the temperature of 80 ℃;
(4) high-temperature calcination: and (4) carrying out high-temperature calcination treatment on the material obtained in the step (3) under the protection of nitrogen. Heating to 400 ℃ at the speed of 2.5 ℃/min, preserving heat for 90min, heating to 800 ℃ at the speed of 4.5 ℃/min, preserving heat for 120min, and then cooling to room temperature to prepare the ultrafast high-adsorption cellulose elastic carbon aerogel.
The performance detection data of the ultrafast high-adsorption cellulose elastic carbon aerogel of the embodiment are as follows: density: 5mg/cm3(ii) a Compressibility: 85 percent; porosity: 92 percent; specific surface area SBET＝682m2(ii)/g; adsorption time for gasoline (90 #): 10 s; the adsorption capacity can reach the self quality160 times the amount.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of ultrafast high-adsorption cellulose elastic carbon aerogel is characterized by comprising the following steps:
(1) and (3) synthesis of bacterial cellulose: inoculating acetobacter xylinum to a fermentation culture medium containing coconuts, and fermenting and biologically synthesizing a bacterial cellulose gel liquid membrane under the conditions of 35-38 ℃ and 40-50% relative humidity RH;
the content of the coconut in the fermentation medium containing the coconut is 20 g/L, wherein the solid content of the coconut is 50-60%;
the fermentation medium comprises peptone 5.0 g/L, yeast extract 5.0 g/L, citric acid 1.0 g/L, and Na2HPO4：3.0g/L，MgSO4：0.4g/L；
The thickness of the bacterial cellulose gel liquid film is 10-20 mm;
(2) freezing and vacuum drying treatment: freezing and solidifying the bacterial cellulose aerogel film obtained in the step (1) by using liquid nitrogen, and then carrying out vacuum drying treatment on the block-shaped module to obtain the bacterial cellulose aerogel;
(3) and (3) PDMS dipping treatment: soaking the bacterial cellulose aerogel obtained in the step (2) in PDMS prepolymer, enabling bubbles in the mixed solution to float to the surface and break by means of vacuumizing, and then putting the mixed solution into an oven;
(4) high-temperature calcination: performing high-temperature calcination treatment on the material obtained in the step (3), and then cooling to obtain ultrafast high-adsorption cellulose elastic carbon aerogel;
the high-temperature calcination treatment is carried out under the protection of nitrogen, the calcination temperature is 500-800 ℃, the temperature is increased to 300-400 ℃ at the speed of 2.0-3.0 ℃/min, the temperature is kept for 60-90 min, then the temperature is increased to the target temperature at the speed of 4-4.5 ℃/min, the temperature is kept for 90-120 min, and then the temperature is reduced to the room temperature.
2. The method for preparing the ultrafast high-adsorbability cellulose elastic carbon aerogel according to claim 1, wherein the method comprises the following steps:
the temperature of the liquid nitrogen freezing and curing treatment in the step (2) is-195 ℃, and the curing time is 10-20 min; the vacuum drying temperature is-45 ℃, the drying time is 60-72 hours, and the vacuum degree is 5-20 Pa.
3. The method for preparing the ultrafast high-adsorbability cellulose elastic carbon aerogel according to claim 1, wherein the method comprises the following steps:
the PDMS prepolymer in the step (3) is a mixture of a silicone rubber prepolymer Sylgard 184 and a curing agent Dow Corning, wherein the weight ratio of 10: 1, mixing; vacuumizing for 30-60 min; thermally curing for 1-4 h in an oven at 60-80 ℃.
4. An ultrafast high-adsorbability cellulose elastic carbon aerogel, which is characterized by being prepared by the preparation method of any one of claims 1 to 3.
5. The ultrafast high-adsorptivity cellulose elastic carbon aerogel according to claim 4, wherein:
the properties of the ultrafast high-adsorption cellulose elastic carbon aerogel are as follows: density: 5-8 mg/cm3(ii) a Compressibility: 78-85%; porosity: 86-92%; specific surface area SBET＝636～682m2(ii)/g; adsorption time for gasoline # 90: 10-30 s; the adsorption capacity can reach 140-160 times of the self mass.
6. The use of the ultrafast high-adsorptivity cellulose elastic carbon aerogel according to claim 4 or 5 for gasoline adsorption.
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